Quillaja-stabilized liquid beverage concentrates and methods of making same

ABSTRACT

Disclosed are stabilized emulsion-including concentrates for drinkable beverages. The emulsion concentrates are stable at pH as low as about 2.0 to about 2.5 and include  quillaja , non-aqueous solvent, acidulant, lipid, and water. The emulsion-including concentrates may remain shelf-stable independently and as part of a drinkable beverage for about twelve months. Methods for making the emulsion-including concentrates are also provided.

CROSS-REFERENCE TO RELATED APPLICATIONS

This application is a divisional of application Ser. No. 14/701,342,filed Apr. 30, 2015, which is incorporated herein by reference in itsentirety.

FIELD

The disclosure relates to liquid beverage concentrates, particularly, toemulsion-including acidic beverage concentrates including a non-aqueousliquid and stabilized with quillaja.

BACKGROUND

Flavored beverages are widely used by consumers and are often preparedusing liquid concentrated drink mixes, including commercially-availableproducts like TANG®, CRYSTAL LIGHT®, and KOOL-AID®, to provide beveragesin a variety of flavors, including fruit and tea flavors. Theingredients of beverage concentrates often contain oils as flavoringagents and are often in a form of an emulsion where the flavor moleculesare suspended within an aqueous medium. Most of the emulsions used inthe beverage industry are oil-in-water emulsions, although there may beadvantages to using other emulsion types for some applications. Flavoredbeverages may also be prepared from frozen, fruit-flavored concentrates,such as those traditionally sold in canisters. Such frozen concentratestypically include a large amount of water and are generally diluted at aratio of 1 part concentrate to 3 parts water to provide the fruitflavored beverage. These types of products are often susceptible tospoilage and require storage at freezer temperatures to provide thedesired shelf life.

A drinkable beverage from a beverage concentrate may be prepared using atwo-step process, where a beverage concentrate including emulsified oilis prepared first, and is then diluted in water to create a drinkablebeverage. Beverage emulsions are considered thermodynamically unstablesystems that tend to break down over time due to a variety ofphysicochemical mechanisms, including gravitational separation,flocculation, coalescence and Ostwald ripening. Beverage emulsions mayinclude weighting agents incorporated into the oil phase to slowgravitational separation of the oil droplets. A number of differentweighting agents are known for utilization within commercial beverageproducts. Such weighting agents include brominated vegetable oil (BVO),sucrose acetate isobutyrate (SAIB), glycerol ester of Wood Rosin (GEWRand also referred to as ester gum), and dammar gum. Drawbacks ofweighting agents such as SAIB, BVO, and GEWR include legal limitsimposed on the amount of such weighting agents that can be added to theemulsions, and the fact that such weighting agents may be perceived bythe consumers as not “natural” and thus undesired.

SUMMARY

Disclosed are quillaja-stabilized emulsion-including acidic beverageconcentrates including a non-aqueous liquid.

In one approach, a concentrate includes about 0.01% to about 10%quillaja; about 15% to about 70% non-aqueous solvent; about 2% to about60% acidulant; about 0.1% to about 20% lipid; and about 1% to about 70%water. The concentrate includes an oil-in-water emulsion and theconcentrate has a pH of about 2.0 to about 2.6 and is shelf-stable atstorage temperatures of about 20° C. to about 25° C. for at least about4 months.

In one approach, a method of making a concentrate including anoil-in-water emulsion includes: providing a solution including about 15%to about 70% non-aqueous solvent and about 2% to about 60% acidulant;mixing quillaja, a lipid, and water to form a blend in a form of anoil-in-water emulsion including about 0.01% to about 20% quillaja, about0.01% to about 60% lipid, about 0% to about 10% buffer, and about 1% toabout 99% water; and adding the blend in an amount of 0.1% to about 35%by total weight to the solution to form an emulsion-includingconcentrate having a pH of about 2.0 to about 2.6.

The concentrate may include 0.05% to about 5% quillaja.

The non-aqueous solvent may be selected from the group consisting ofpropylene glycol, glycerol, ethanol, triacetin, ethyl acetate, benzylalcohol, vegetable oil, 1,3-propanediol, and combinations thereof.

The acidulant may be selected from the group consisting of citric acid,malic acid, succinic acid, acetic acid, adipic acid, tartaric acid,fumaric acid, phosphoric acid, lactic acid, salts thereof, andcombinations thereof.

The lipid may be elected from the group consisting of castor oil,terpene hydrocarbons, flavor oils (consisting of one or more of thefollowing derivatives: ketones, aldehydes, lactones, ethers, esters,sulfur compounds, furanones, terpenoids), oil soluble vitamins,nutraceuticals, fatty acids, poly-unsaturated fatty acids, triglyceridesand triglyceride derivatives, antioxidants, colorants, vegetable oils,and combinations thereof.

The concentrate may have a ratio of the water to the non-aqueous solventin the concentrate is from about 6:1 to about 1:6 and a ratio of thewater to the acidulant in the concentrate is from about 60:1 to about1:10.

The buffer may be selected from the group consisting of sodium, calciumor potassium salts of citrate, malate, succinate, acetate, adipate,tartrate, fumarate, phosphate, lactate, or carbonate, and combinationsthereof.

The concentrate may include water in an amount of 30% or less.

In one approach, the concentrate does not include a weighting agent.

The concentrate may be shelf-stable at storage temperatures of about 20°C. to about 25° C. for about twelve months.

DETAILED DESCRIPTION

Quillaja is an organic/natural surfactant extracted from the bark of theQuillaja saponaria tree. It is known for its use as a foam stabilizerand an emulsifier for oil-in-water emulsions. Quillaja is known tocontain surface active components that are capable of forming surfactantmicelles and stabilizing oil-in-water emulsions and can be used to formemulsions containing small droplets that are stable to changes in pH,ionic strength, and temperature. When quillaja is used as an emulsifier,it is believed to stabilize a beverage emulsion through electrostaticrepulsion (i.e. negatively-charged functional groups within theemulsifier). Other types of emulsifiers such as gum acacia stabilize oildroplets through negatively-charged electrostatic repulsion and sterichindrance. Quillaja has been found to be stable in products stored atambient (20° C.-25° C.) temperatures for up to a year. One advantage ofquillaja over gum acacia is that, due to quillaja's ability to stabilizesmall oil droplet size, unlike gum acacia, quillaja may not need aweighting agent such as BVO, SAIB, or GEWR (ester gum) to stabilize theemulsion. Another advantage of quillaja is that, when used in a beverageapplication, quillaja is typically considered by the beverage industryas a “natural flavor” unlike many other beverage emulsifiers such as gumacacia, modified food starch, polysorbate 60, DATEM, and the like.

One known disadvantage of using quillaja in beverage concentrateemulsions is that, when the pH of the aqueous phase of the emulsiondrops under approximately 2.6, quillaja is believed to lose its negativecharges due to the protonation of the negative functional groups ofquillaja by the free hydrogens of the acidulants present in theconcentrate. This is believed to cause quillaja to no longer tostabilize the emulsion through electrostatic repulsion. Thequillaja-stabilized oil droplets may then be permitted to aggregatetogether, possibly coalesce (i.e., one or more smaller droplets may fuseinto one or more larger droplets), and cream (i.e., float upward) to thesurface of the liquid concentrate and/or the finished beverage, which isconsidered undesirable. To date, there is no known method to stabilizequillaja for a beverage application with a pH under 2.6.

Generally, emulsion-including beverage concentrates described hereininclude quillaja that provides enhanced stability to the ingredients ofthe beverage concentrates. More particularly, the emulsion-includingbeverage concentrates including quillaja as described herein provideenhanced flavor stability despite a low pH (i.e., from about 2.0 toabout 2.6). In one aspect, at least some of the water in the emulsionbeverage concentrates is replaced with a non-aqueous solvent,advantageously restricting the protonation of the quillaja by theacidulants present in the beverage concentrates. While the disclosure isprimarily directed to the use of emulsion concentrates for providingflavored beverages, the use of the emulsion concentrates to provideflavor to a variety of food products is also contemplated. In someapproaches, the emulsion concentrates disclosed herein remainshelf-stable for up to about twelve months and can be diluted to prepareflavored beverages with desired flavor profiles and with little or noflavor degradation.

As used herein, the term “concentrate” means a liquid composition thatcan be diluted with an aqueous, potable liquid to provide a beverage oradded to a food product prior to being consumed. The phrase “liquid”refers to a non-gaseous, flowable, fluid composition at room temperature(i.e., about 20° C. to about 25° C.). By “shelf-stable,” it is meantthat the concentrate avoids substantial flavor degradation and ismicrobially stable such that the concentrate has an aerobic plate count(APC) of less than about 5000 CFU/g, yeast and mold at a level less thanabout 500 CFU/g, and coliforms at 0 MPN/g for at least about six months,in another aspect at least about eight months, in another aspect atleast about ten months, and in yet another aspect at least about twelvemonths, when stored at e room temperature in a sealed container. In someapproaches, “enhanced flavor stability” and “avoiding substantialdegradation of flavor” means that the emulsion concentrates describedherein retain more flavor after storage at room temperature over theshelf life of the product as compared to an otherwise identicalconcentrate including water instead of a combination of water and anon-aqueous solvent. In other approaches, “enhanced flavor stability”and “avoiding substantial degradation of flavor” means that there islittle change in flavor and development of off flavor in the concentratewhen stored at room temperature over the shelf life of the product in asealed container.

In various aspects, the beverage concentrates as described herein areoil-in-water emulsions having a pH of below about 2.6, and in othercases, from about 2.0 to about 2.6, and include about 0.01% to about 10%quillaja; about 15% to about 70% non-aqueous solvent; about 2% to about60% acidulant; about 0.1% to about 20% lipid; and about 1% to about 70%water. By virtue of balancing the amount of non-aqueous liquid, water,and acidulants in the system, the emulsion-including beverageconcentrates described herein advantageously contain less dissociatedacid and have less quillaja degradation, which provides for enhancedstabilization of the emulsion concentrates in comparison to otherwiseidentical concentrates including only water and no non-aqueous liquid.

The emulsion-including beverage concentrates may include about 0.01% toabout 8% quillaja in one approach, about 0.05% to about 5% quillaja inanother approach, and about 0.075% to about 3.5% quillaja in yet anotherapproach. In one aspect, due to the use of quillaja as an emulsifier,the emulsion concentrates described are substantially free of weightingagents, thereby advantageously lowering manufacturing costs. Withoutwishing to be limited by theory, the emulsions as described herein maybe substantially free of a weighting agent due to the ability ofquillaja to stabilize small oil droplets. As used herein, the term“substantially free of” means that a component is entirely absent or ispresent in an amount of up to about 0.05%, up to about 0.1%, or up toabout 0.5% by total weight of the composition. Structurally, quillajahas negative charges that provide for its emulsion-stabilizing effectvia electrostatic repulsion. While quillaja typically loses its negativecharges due to protonation of the functional groups of quillaja by thefree hydrogen of the present acidulants, which causes quillaja to nolonger to stabilize the emulsion through electrostatic repulsion, thepresence of a non-aqueous solvent in the emulsion-including beverageconcentrates as described herein advantageously associates with the acidpresent in the concentrate and restricts and/or eliminates thede-protonation of the acid, permitting quillaja to maintain its negativecharges and stability.

In other aspects, the acidulant or acidulants provided in theemulsion-including beverage concentrates described herein may beselected from the group consisting of citric acid, malic acid, succinicacid, adipic acid, tartaric acid, fumaric acid, phosphoric acid, lacticacid, salts thereof, and combinations thereof. By one approach, theselection of the acidulant used in various embodiments of the beverageconcentrates described herein can provide substantially improved flavorand decreased aftertaste, particularly when the concentrate is dosed toprovide a final beverage with greater than typical amounts of thebeverage concentrate. In some aspects, the selection of the acidulantmay depend, at least in part, on the desired pH of the concentrateand/or taste imparted by the acidulant to the diluted final beverage. Inanother aspect, the amount of acidulant included in the concentrate maydepend on the strength of the acid. For example, a larger quantity oflactic acid would be needed in the concentrate to reduce the pH in thefinal beverage than a stronger acid, such as phosphoric acid.

In various beverage concentrate applications, it may be desirable toinclude acidulant in the concentrate so that a flavored beverage madetherefore has a tart flavor that enhances the overall flavor profile ofthe beverage. For example, it may be desirable to provide alemon-flavored beverage that has a tart flavor similar to that of alemonade drink made with fresh lemons. A variety of other flavors canalso be enhanced by a tart flavor, such as other fruit flavors. In someapproaches, the liquid concentrates provided herein include asubstantial acidulant content. In one aspect, the beverage concentrateincludes at least about 3% to about 60% acidulant in one aspect, inanother aspect about 5% to about 45% percent acidulant, in yet anotheraspect about 7.5% to about 45% percent acidulant, and in still anotheraspect about 10% to about 35% percent acidulant by weight of theconcentrate.

In other aspects, the lipid or lipids provided in the emulsion-includingbeverage concentrates described herein may be selected from the groupconsisting of castor oil, terpene hydrocarbons, flavor oils (possiblyconsisting of the following types of molecules: ketones, aldehydes,lactones, ethers, esters, sulfur compounds, furanones, terpenoids), oilsoluble vitamins, nutraceuticals, fatty acids, poly-unsaturated fattyacids, triglycerides and triglyceride derivatives, antioxidants,colorants, vegetable oils, and combinations.

In some aspects, the emulsion-including beverage concentrates describedherein include water in an amount of about 1 to about 70 percent, inanother aspect from about 5 percent to about 45 percent, in anotheraspect about 10 percent to about 40 percent water. For purposes ofcalculating the water content of the emulsion beverage concentratesdescribed herein, the amount of water in a concentrate includes waterincluded as a separate ingredient as well as any water provided in anyingredients used in the concentrate. In at least some aspects, thepresence of water in any form is minimized to the extent practical.Without wishing to be limited by theory, inclusion of large amounts ofwater in emulsion-including beverage concentrates can be problematic fora number of reasons, including, for example: (1) supporting growth ofmicrobes, such as yeast, mold, and bacteria; (2) facilitating hydrolysisof flavor components and other unwanted chemical reactions; and (3)limiting the amount of flavoring or other ingredients that can bedissolved in the concentrate. Furthermore, high water content can alsobe detrimental to the emulsion when acidulants are included in theemulsion due to lowering of pH and resulting instability of someingredients at low pH.

For example, some flavorings, sweeteners, vitamins, and/or coloringredients are rapidly degraded in water or an acidic environment,thereby limiting the types of flavorings that are suitable for inclusionin water-based beverage concentrates or ready-to-drink beverages. Forinstance, some flavor degradation reactions require the presence ofwater while others require protons from dissociated acids. Certain typesof flavorings, such as acid labile citrus flavorings including terpenesand sesquiterpenes, have greater susceptibility to degradation, andproducts including them typically have very short shelf lives (even amatter of days) when stored above refrigeration temperatures due todevelopment of off-flavor notes and alteration of the taste profile ofthe product. Exemplary other ingredients exhibiting instability in waterand/or at low pH include, for example, vitamins, particularly vitaminsA, C, and E; high potency sweeteners (such as, for example, monatin,neotame, Luo Han Guo), colorants (such as for example fruit andvegetable extracts, anthocyanins, copper chlorophyllin, curcumin,riboflavin), sucrose, proteins, hydrocolloids, starch, and fiber. Thesetypes of ingredients can advantageously be included in theemulsion-including beverage concentrates described herein and exhibitimproved stability when stored at room temperatures compared tootherwise identical concentrates having higher amounts of water and nonon-aqueous solvent.

The emulsion-including beverage concentrates may include about 15% toabout 70% non-aqueous liquid in one approach, about 20% to about 60%non-aqueous liquid in another approach, and about 25% to about 50%non-aqueous liquid in yet another approach. Exemplary non-aqueousliquids include, but are not limited to, propylene glycol, glycerol,triacetin, ethanol, ethyl acetate, benzyl alcohol, vegetable oil,vitamin oil (e.g., Vitamin E, Vitamin A), 1,3-propanediol, andcombinations thereof. In one aspect, selection of the non-aqueous liquidfor use in the beverage concentrates may depend, at least in part, onthe ability of the non-aqueous liquid to solubilize other ingredients ofthe concentrate or to form an emulsion with another non-aqueous liquid.

For example, sucralose, a high intensity sweetener, is more readilysolubilized in 1,3-propanediol than in propylene glycol. Therefore,beverage concentrates including sucralose may be advantageously preparedusing a solvent comprising 1,3-propanediol to provide a beverageconcentrate that is able to maintain sucralose in solution throughoutits shelf life. In other instances, selection of the non-aqueous liquidmay also depend, at least in part, on the flavor provided by thenon-aqueous liquid and the desired taste profile in the final beverage.In yet other instances, selection of the non-aqueous liquid may alsodepend, at least in part, on the viscosity and/or the desired density ofthe resulting concentrate.

In some aspects, the emulsion concentrates may have a ratio of the waterto the non-aqueous solvent from about 7:1 to about 1:5 in one aspect,from about 4:1 to about 1:4 in another aspect, from about 3:1 to about1:3 in yet another aspect, and from about 1:2 to about 2:1 in stillanother aspect.

In some aspects, the emulsion concentrates may have a ratio of thequillaja to the non-aqueous solvent from about 1:1500 to about 1:2 inone aspect, from about 1:900 to about 1:5 in another aspect, from about1:850 to about 1:20 in yet another aspect, and from about 1:750 to about1:50 in still another aspect.

As described in more detail in U.S. application Ser. No. 13/416,671filed Mar. 9, 2012, which is incorporated by reference herein in itsentirety, acidulants typically have lower acid dissociation constants(K_(a)) in organic liquids (such as non-aqueous liquids) than in water.For instance, the K_(a) value for a particular acidulant may be, forexample, several orders of magnitude or more lower in a non-aqueousliquid than in water. If the acidulant is dissolved in a mixture ofwater and a particular non-aqueous liquid, its resulting K_(a) valuewould generally be intermediate between its K_(a) values in pure waterand pure non-aqueous liquid, and its exact K_(a) value would be relatedto the ratio of water to non-aqueous liquid in the mixture.

For example, an acidulant having a K_(a) value equal to about 10⁻³ (anda pK_(a) value, defined as (−log₁₀K_(a)), equal to about 3) in watermight have a K_(a) value equal to about 10⁻⁸ (and a pK_(a) value equalto about 8) in a particular non-aqueous liquid/solvent, such aspropylene glycol. Accordingly, the K_(a) value corresponding to theextent of acid dissociation occurring in the acidulant would be expectedto be about five orders of magnitude lower (about 100,000 times lower)in the particular non-aqueous liquid than in water. Further, if theacidulant is dissolved in a mixture of water and a particularnon-aqueous liquid, its resulting K_(a) value would generally beintermediate between its K_(a) values in pure water and pure non-aqueousliquid, and its exact K_(a) value would be related to the ratio of waterto non-aqueous liquid in the mixture. In general, the relationshipbetween the acidulant K_(a) value and the composition of liquid in whichthe acidulant is dissolved is logarithmic in nature. Therefore,replacing even small proportions of water with one or more non-aqueousliquid advantageously produces substantial reductions in the acidulantK_(a) value and extent of acid dissociation in a liquid mixture. Forexample, replacing about half the water in the concentrate with anon-aqueous liquid may reduce the acidulant K_(a) value and extent ofacid dissociation in a liquid mixture by many hundred-fold, manythousand-fold, many million-fold, or more depending on the compositionof the non-aqueous liquid(s) and the proportion of water in the liquidmixture.

The non-aqueous liquids utilized in the beverage concentrates describedherein may be either protic or aprotic. As used herein, proticnon-aqueous liquids possess one or more hydroxyl group having anionizable hydrogen atom, while aprotic non-aqueous liquids do not.Protic non-aqueous liquids that are particularly suited because of theirgenerally bland flavor and compatibility with foods include, forexample, glycerol, propylene glycol, and 1,3-propanediol. Aproticnon-aqueous liquids that may be utilized for generally the same reasonsinclude, for example, triacetin and vegetable oils, such as coffee oilor medium-chain triglyceride oils. In general, food acids dissolved inaprotic non-aqueous liquids will dissociate to a lesser extent than thesame acids dissolved in protic non-aqueous liquids, and acids dissolvedin non-aqueous liquid mixtures will dissociate to intermediate extentsin general proportion to the compositions and levels of non-aqueousliquids present. The non-aqueous liquids can be selected toadvantageously control extent of acid dissociation and pH of thebeverage concentrates created using acidic flavor sources and/or addedacids.

Because non-aqueous liquids typically have higher solventself-dissociation constants than water, acidulants dissolved innon-aqueous liquids have higher pH values than acidulants dissolved inwater. Even though an acidulant may completely dissolve in a non-aqueousliquid, it is believed that protons present in the acidulant's carboxylgroups may not dissociate or weakly dissociate (relative to theirdissociation in water)—or may dissociate but remain in close proximityto carboxyl anions—to beneficially lower the free proton concentrationand thereby lower the potential to cause or promote chemical reactionsin the concentrate. Further, the lower water content in the beverageconcentrates described herein reduces or prevents formation of highlyreactive, strongly acidic hydronium ions that are present in acidifiedaqueous solutions. Therefore, the formation of hydronium ions is higherin concentrates including higher amounts of water and lesser amounts ofnon-aqueous liquid. Lower K_(a) values and the resulting free protonconcentration in the liquid beverage concentrates provided herein arebelieved to greatly slow or prevent unwanted chemical reactions, therebyimproving flavor stability and product shelf-life despite the relativelyhigh acidulant content.

In some aspects, the concentrated flavor composition may further includea sweetener. Useful sweeteners may include both nutritive andnon-nutritive sweeteners, including both low intensity and highintensity sweeteners, such as, for example, honey, corn syrup, highfructose corn syrup, erythritol, sucralose, aspartame, stevia,saccharine, monatin, luo han guo, neotame, sucrose, Rebaudioside A(often referred to as “Reb A”), fructose, cyclamates (such as sodiumcyclamate), acesulfame potassium, and combinations thereof. Theselection of sweetener and amount of sweetener added may depend, atleast in part, on the desired viscosity of the concentrated flavorcomposition. For example, nutritive sweeteners like sucrose may beincluded in much higher amounts than high intensity sweeteners likeneotame to provide the same level of sweetness and such higher totalsolids content contributed by the sweetener increases the viscosity ofthe composition. If desired, the sweetener can generally be added in anamount of about 0.2 to about 60 percent, with the lower end of the rangegenerally more appropriate for high intensity sweeteners and the upperend of the range generally more appropriate for nutritive sweeteners.

In some aspects, the concentrates may further include from about 0% toabout 20% buffer in one approach, from about 0% to about 15% buffer inanother approach, from about 0% to about 10% buffer in yet anotherapproach, and from 0% to about 5% buffer in still another approach. Forconcentrates having lower water content, such as less than about 15percent, buffer may be included for primarily flavor purposes. Forconcentrates having higher water content, such as about 15 to about 30percent water, buffer may be included in an amount relative to theacidulant content. For example, the acid:buffer ratio can be about 1:1to about 25,000:1, in another aspect about 1.25:1 to about 4000:1, inanother aspect about 1.7:1 to about 3000:1, and in another aspect about2.3:1 to about 250:1. In this respect, a buffered concentrate mayinclude more acidulant and can be diluted to provide a final beveragewith enhanced tartness due to increased acidulant content as compared toa beverage provided from an otherwise identical concentrate at the samepH but which lacks buffers. Inclusion of buffers may also beadvantageous to the flavor profile in the resulting final beverage.

Suitable buffers include, for example, a conjugated base of an acid(e.g., sodium citrate and potassium citrate), acetate, phosphate or anysalt of an acid. In other instances, an undissociated salt of the acidcan buffer the concentrate. In some approaches, the buffer may beselected from a group consisting of sodium, calcium or potassium saltsof citrate, malate, succinate, acetate, adipate, tartrate, fumarate,phosphate, lactate, or carbonate, and combinations thereof.

The concentrates described herein may be provided with a variety ofdifferent flavors, such as, for example, fruit flavors, tea flavors,coffee flavors, and combinations thereof. Flavorings useful in theliquid concentrates described herein may include, for example, liquidflavorings (including, for example, alcohol-including flavorings (e.g.,flavorings including ethanol, propylene glycol, 1,3-propanediol,glycerol, and combinations thereof), and flavor emulsions (e.g., nano-and micro-emulsions)) and powdered flavorings (including, for example,extruded, spray-dried, agglomerated, freeze-dried, and encapsulatedflavorings). The flavorings may also be in the form of an extract, suchas a fruit extract. The flavorings can be used alone or in variouscombinations to provide the concentrate with a desired flavor profile.The flavorings can be included at about from about 0.01 percent to about10 percent in one aspect, from about 0.05 percent to about 8 percent inanother aspect, from about 0.75 percent to about 7 percent in yetanother aspect, and from about 0.1 percent to about 6 percent in stillanother aspect.

In another aspect, a variety of different alcohol-including flavoringsmay be included in the concentrated composition. The alcohols typicallyused in commercially available flavorings include compounds having oneor more hydroxyl groups, including ethanol and propylene glycol,although others may be used, if desired. The flavoring may also include1,3-propanediol, if desired. Suitable alcohol-including flavoringsinclude, for example, lemon, lime, cranberry, apple, watermelon,strawberry, pomegranate, berry, cherry, peach, passionfruit, mango,punch, white peach tea, sweet tea, and combinations thereof.

Optionally, colors can be included in the liquid beverage concentrates.The colors can include artificial colors, natural colors, or acombination thereof.

Optionally, the concentrated flavor compositions can further includesalts, preservatives, viscosifiers, surfactants, stimulants,antioxidants, caffeine, electrolytes (including salts), nutrients (e.g.,vitamins and minerals), stabilizers, gums, and the like. Preservatives,such as EDTA, sodium benzoate, potassium sorbate, sodiumhexametaphosphate, nisin, natamycin, polylysine, and the like can beincluded, if desired. Exemplary salts include, for example, sodiumcitrate, mono sodium phosphate, potassium chloride, magnesium chloride,sodium chloride, calcium chloride, the like, and combinations thereof.

In various approaches, the beverage concentrates described herein may beformulated to be diluted by a factor of at least 25 times to provide afinal beverage, which can be, for example, an 8 ounce beverage. By someapproaches, the beverage concentrate can be provided at a concentrationof about 25 to about 500 times, in another aspect about 25 to about 225times, in another aspect about 50 to about 200 times, in another aspectabout 75 to about 160 times, and in yet another aspect about 90 to about120 times that needed to provide a desired level of flavor intensity,acidity, and/or sweetness to a final beverage, which can be, forexample, an 8 ounce beverage. The term “final beverage” as used hereinmeans a beverage that has been prepared by diluting the beverageconcentrate to provide a beverage in a potable, consumable form. By wayof example, to clarify the term “concentration,” a concentration of 75times (i.e., “75×”) would be equivalent to 1 part concentrate to 74parts water (or other potable liquid) to provide the final beverage. Inother words, the flavour profile of the final beverage is taken intoaccount when determining an appropriate level of dilution, and thusconcentration, of the emulsion-including beverage concentrate. Thedilution factor of the beverage concentrate can also be expressed as theamount necessary to provide a single serving of concentrate.

Because of the high concentration factor (i.e., at least about 25×) ofthe beverage concentrates provided herein, large amounts of acidulant(i.e., at least about 5 percent) are included in the concentrates toprovide the desired tartness in the final beverage. It was surprisinglyfound that a large quantity of acidulant could be included in thebeverage concentrates in the amount necessary to provide a tart flavorwhen diluted to provide a final beverage but without detrimentallyaffecting the stabilizing function of quillaja or the stability of theflavor ingredients. The emulsion-including beverage concentrates asdescribed herein have high acidulant content and due at least to thepresent of the non-aqueous solvent are advantageously characterized byreduced production of off-flavor notes and reduced degradation of addedcoloring and/or sweeteners, particularly high intensity sweeteners,during storage at room temperature as compared to otherwise identicalbeverage concentrates with higher water content. More specifically, byvirtue of balancing the amount of non-aqueous liquid, water, acidulant,quillaja and lipid in the system, the liquid beverage concentratecontains less dissociated acid and has less flavor degradation after,for example, twelve months storage at room temperature in comparison toan otherwise identical concentrate including water instead ofnon-aqueous liquid.

The emulsion-including beverage concentrates as described herein can beprepared by a variety of processes. Concentrates in the form ofemulsions, solutions (i.e., in which the ingredients are dissolved inthe non-aqueous liquid), and suspensions can be prepared by the methodsdescribed below. The concentrates described herein can include bothwater-soluble and water-insoluble ingredients, as well as ingredientsthat are soluble and insoluble in the selected non-aqueous liquid. Othermethods of preparing the liquid concentrates having low water content asdescribed herein can also be used, if desired. The following methods areintended to be exemplary but not limiting in scope.

In one aspect, a beverage concentrate is provided in the form of asolution. In this respect, a method is provided for preparing a beverageconcentrate in the form of an oil-in-water emulsion, the methodcomprising providing a solution including about 15% to about 70%non-aqueous solvent and about 3% to about 50% acidulant; mixingquillaja, a lipid, and water to form a blend in a form of anoil-in-water emulsion including about 0.01% to about 20% quillaja, about0.01% to about 60% lipid, and about 1% to about 99% water; and addingthe blend in an amount of 0.1% to about 35% by total weight to thesolution to form an emulsion-including beverage concentrate having a pHof about 2.0 to about 2.6.

The beverage concentrates described herein can also be added to potableliquids to form flavored beverages. In some aspects, theemulsion-including beverage concentrate may be non-potable (such as dueto the high acid content and intensity of flavor). For example, thebeverage concentrate can be used to provide flavor to water, cola,carbonated water, tea, coffee, seltzer, club soda, the like, and canalso be used to enhance the flavor of juice. In one aspect, the beverageconcentrate can be used to provide flavor to alcoholic beverages,including but not limited to flavored champagne, sparkling wine, winespritzer, cocktail, martini, or the like. By some approaches, theconcentrate can be added to the potable liquid without stirring.

The concentrates described herein can be combined with a variety of foodproducts to add flavor to the food products. For example, theconcentrates described herein can be used to provide flavor to a varietyof solid, semi-solid, and liquid food products, including but notlimited to oatmeal, cereal, yogurt, strained yogurt, cottage cheese,cream cheese, frosting, salad dressing, sauce, and desserts such as icecream, sherbet, sorbet, and Italian ice. Appropriate ratios of thebeverage concentrate to food product or beverage can readily bedetermined by one of ordinary skill in the art.

The emulsion-including beverage concentrates as described herein may bepackaged as follows. Some conventional beverages and beverageconcentrates, such as juices, may be hot filled (for example, at 93° C.)during packaging and then sealed to prevent microbial growth. Thebeverage concentrates provided herein, given a combination of thenon-aqueous liquid content, acidulant content, and low water activity,do not require thermal treatments or mechanical treatments, such aspressure or ultrasound, to reduce microbial activity either before orafter packaging. By one approach, the beverage concentrates areadvantageously suitable for cold filling while maintaining shelfstability for at least about three months, in another aspect at leastabout six months, in another aspect at least about eight months, inanother aspect at least about ten months, and in another aspect at leastabout twelve months at room temperature. The packaging for theconcentrates generally does not require additional chemical orirradiation treatment. The product, processing equipment, package andmanufacturing environment need not be subject to aseptic packagingpractices. As such, the concentrates described herein can allow forreduced manufacturing costs.

The concentrated beverage liquids described herein can be used with avariety of different types of containers. One exemplary container isdescribed in WO 2011/031985, which is incorporated herein by referencein its entirety. Other types of containers can also be used, if desired.In one aspect, the liquid beverage concentrates may be packaged incontainers in an amount of about 0.5 to about 6 oz. of concentrate, inanother aspect of about 1 to about 4 oz., and in another aspect about 1to about 2 oz., with the quantity being sufficient to make at leastabout 10 eight oz. servings of a final flavored beverage.

Advantages and embodiments of the concentrate compositions describedherein are further illustrated by the following examples; however, theparticular conditions, processing schemes, materials, and amountsthereof recited in these examples, as well as other conditions anddetails, should not be construed to unduly limit the compositions andmethods described herein. All percentages in this application are byweight unless otherwise indicated.

EXAMPLES

The Examples below evaluate stability of the samples using aninstability index that measures the overall degree of creaming of theentire sample. For purposes of this application, the instability indexmeasures how much an oil droplet creamed or sedimented over a period oftime in an aqueous solution. An instability index of 0 indicates nocreaming while an instability index of 1 indicates complete creaming.

In the examples below, the emulsions were produced with a Silverson L4RHigh Shear Mixer with Silverson's Fine Emulsor Stator at 70° F. Thesamples were homogenized at ⅔ of the L4R's capacity speed for about 5minutes. The samples in the examples below were analyzed by thedispersion analyzer LUMiSizer® (manufactured by LUM GmbH, Berlin,Germany) as emulsion concentrates. The software program of theLUMiSizer® was SEPView™ 6.1.2657.8312. Without wishing to be limited bytheory, since creaming of the emulsions is due to gravity, theLUMiSizer® increases gravitational forces to accelerate creaming atvarious RCF values. The relative centrifugation force (RCF) will beunderstood to mean will be understood as amount of times the forceprovided by the machine is stronger than the earth's gravity.

The sample volumes were 1.5 ml and LUM 10.0 mm vials (polycarbonatesynthetic cell, [110-132xx]) were used. The standard operating procedureused to generate the data in the examples below was as follows: speed of2700 RPM, light factor of 1.0, temperature of 25.0° C., using 60measurements and intervals being of 30 seconds and 60 additionalmeasurements at intervals of 60 seconds.

Example 1

Procedure: an emulsion concentrate including 5% Quillaja, 10% CastorOil, 84.95% Water, and 0.05% Potassium Sorbate was made using a HighShear Silverson Mixer L4R with Silverson's Fine Emulsor Stator at 70°F., by mixing for 5 minutes at ⅔ Speed. The emulsion concentrate wasthen added at 10% (w/w) to systems including 20% malic acid (w/w), 1.5%potassium citrate (w/w) and 68.5% total solvent (w/w). The total solventlevels were the following: 68% water (Sample A), 34% water and 34%glycerin (Sample B), 15% water and 53% glycerin (Sample C), 10% waterand 58% glycerin (Sample D), 5% water and 63.5% glycerin (Sample E).

The samples were run at 2700 RPM in the LUMiSizer® for 500 seconds atapproximately 970-980 g and were measured by the LUMiSizer® in the rangeof 17.51 mm (from 111.10 mm to 128.61 mm). The pH (reported by BrinkmannMetrohm pH meter 6.3026.250 and probe 6.0259.100 instrument[standardized per machine's protocol with pH 2, 4, and 7 buffersolutions]) and instability index (calculated and reported by theLUMiSizer®) of the samples were as follows:

TABLE 1 Instability Sample Name pH Index Sample A (0.5% Quillaja 1%Castor 2.10 0.54 Oil; 68% Water) Day 1 Sample B (0.5% Quillaja 1% CastorOil; 2.20 0.29 34% Water; 34% Glycerin) Day 1 Sample C (0.5% Quillaja 1%Castor Oil; 2.25 0.25 15% Water; 53% Glycerin) Day 1 Sample D (0.5%Quillaja 1% Castor 2.28 0.21 Oil; 10% Water; 58% Glycerin) Day 1 SampleE (0.5% Quillaja 1% Castor Oil; 2.33 0.18 5% Water; 53% Glycerin) Day 1

It was observed that as more water was replaced with glycerin, thequillaja showed increasingly enhanced stability relative to the control(Sample A) due to glycerin's effect on the acidulants.

Example 2

The samples were prepared using the ingredients and procedure of Example1, but the acidulants and buffer (i.e., malic acid and potassiumcitrate) were replaced with sucrose, a chemical that has no impact onelectrostatic repulsion. The samples were run at 2700 RPM in theLUMiSizer® for 500 seconds at approximately 970-980 g and were measuredby the LUMiSizer® in the range of 14.86 mm (from 111.10 mm to 125.96mm). The pH (reported by Brinkmann Metrohm pH meter 6.3026.250 and probe6.0259.100 instrument [standardized per machine's protocol with pH 2, 4,and 7 buffer solutions]) and instability index (calculated and reportedby the LUMiSizer®) of the samples were as follows:

TABLE 2 Instability Sample Name pH Index Sample A (0.5% Quillaja 1%Castor 4.55 0.16 Oil; 68% Water) Day 2 Sample B (0.5% Quillaja 1% Castor4.73 0.21 Oil; 34% Water 34% Glycerin) Day 1 Sample C (0.5% Quillaja 1%Castor 4.80 0.18 Oil; 15% Water 53% Glycerin) Day 1 Sample (0.5%Quillaja 1% Castor 4.83 0.16 Oil; 10% Water 58% Glycerin) Day 1 Sample E(0.5% Quillaja 1% Castor 4.83 0.14 Oil; 5% Water 63% Glycerin) Day 1

The high instability index value (0.54) of the control Sample A inExample 1 was determined to be due to the presence of the acidulants,and Example 2 shows that when the acidulants were replaced with sucrose,the instability index of Sample A was substantially lower (0.16), whichwas in line with the instability indexes of the glycerin-includingSamples B-E of Example 1.

Example 3

The samples were prepared using the ingredients and procedure of Example1, but the instability index was measured on day 4 after storage of theconcentrates at 70° F.). Sample A was not run due to destabilization onday 1. The samples were run at 2700 RPM in the LUMiSizer® for 500seconds at approximately 970-980 g and were measured by the LUMiSizer®in the range of 17.55 mm (from 111.29 mm to 128.84 mm). The instabilityindex (calculated and reported by the LUMiSizer®) of the samples wasfollows:

TABLE 3 Instability Sample Name Index Sample B (0.5% Quillaja 1% CastorOil, 0.29 34% Water 34% Glycerin 20% Acid) Day 4 Sample C (0.5% Quillaja1% Castor Oil, 0.25 15% Water 53% Glycerin 20% Acid) Day 4 Sample D(0.5% Quillaja 1% Castor Oil, 0.17 10% Water 58% Glycerin 20% Acid) Day4 Sample E (0.5% Quillaja 1% Castor Oil, 0.17 5% Water 63% Glycerin 20%Acid) Day 4

It was observed that the concentrate had comparable (if not identical)instability index on day 4 as on day 1.

Example 4

The samples were prepared using the ingredients and procedure of Example1, but medium chain triglycerides (MCT) were used in the place of castoroil. The samples were run at 2700 RPM in the LUMiSizer® for 150 secondsat approximately 970-980 g and were measured by the LUMiSizer® in therange of 16.75 mm (from 111.34 mm to 127.09 mm). The pH (reported byBrinkmann Metrohm pH meter 6.3026.250 and probe 6.0259.100 instrument[standardized per machine's protocol with pH 2, 4, and 7 buffersolutions]) and instability index (calculated and reported by theLUMiSizer®) of the samples were as follows:

TABLE 4 Instability Sample Name pH Index Sample A (0.5% Quillaja 1% MCT,2.10 0.64 68% Water 20% Acid) Day 1 Sample B (0.5% Quillaja 1% MCT, 2.200.58 34% Water 34% Glycerin 20% Acid) Day 1 Sample C (0.5% Quillaja 1%MCT, 2.26 0.16 10% Water 58% Glycerin 20% Acid) Day 1 Sample D (0.5%Quillaja 1% MCT, 2.28 0.15 5% Water 63% Glycerin 20% Acid) Day 1 SampleE (0.5% Quillaja 1% MCT, 2.33 0.14 15% Water 53% Glycerin 20% Acid) Day1

This Example shows that even when castor oil is replaced with anotherlipid such as medium chain triglycerides, as more water was replacedwith glycerin, the quillaja showed increasingly enhanced stabilityrelative to the control (Sample A) due to glycerin's effect on theacidulants.

Example 5

The samples were prepared using the ingredients and procedure of Example1, but terpene hydrocarbons were used in the place of castor oil. Thesamples were run at 2700 RPM in the LUMiSizer® for 500 seconds atapproximately 970-980 g and were measured by the LUMiSizer® in the rangeof 17.38 mm (from 110.91 mm to 128.29 mm). The pH (reported by BrinkmannMetrohm pH meter 6.3026.250 and probe 6.0259.100 instrument[standardized per machine's protocol with pH 2, 4, and 7 buffersolutions]) and instability index (calculated and reported by theLUMiSizer®) of the samples were as follows:

TABLE 5 Instability Sample Name pH Index Sample A (0.5% Quillaja 1%Terpene 2.10 0.77 Hydrocarbons 34% Water 34% Glycerin 20% Acid) Day 1Sample B (0.5% Quillaja 1% Terpene 2.21 0.74 Hydrocarbons 68% Water 20%Acid) Day 1 Sample C (0.5% Quillaja 1% Terpene 2.24 0.51 Hydrocarbons15% Water 53% Glycerin 20% Acid) Day 1 Sample D (0.5% Quillaja 1%Terpene 2.27 0.40 Hydrocarbons 10% Water 58% Glycerin 20% Acid) Day 1Sample E (0.5% Quillaja 1% Terpene 2.34 0.26 Hydrocarbons 5% Water 53%Glycerin 20% Acid) Day 1

This Example shows that as castor oil is replaced with another lipidsuch as terpene hydrocarbons, as more water was replaced with glycerin,the quillaja showed increasingly enhanced stability relative to thecontrol (Sample A) due to glycerin's effect on the acidulants.

Example 6

The samples were prepared using the ingredients and procedure of Example1, but propylyne glycol (PG) was used in the place of glycerin. Thesamples were run at 2700 RPM in the LUMiSizer® for 500 seconds atapproximately 970-980 g and were measured by the LUMiSizer® in the rangeof 16.33 mm (from 111.73 mm to 128.06 mm). The pH (reported by BrinkmannMetrohm pH meter 6.3026.250 and probe 6.0259.100 instrument[standardized per machine's protocol with pH 2, 4, and 7 buffersolutions]) and instability index (calculated and reported by theLUMiSizer®) of the samples were as follows:

TABLE 6 Instability Sample Name pH Index Sample A (0.5% Quillaja 1%Castor, 68% 2.13 0.55 Water with 0% PG) Day 1 Sample B (0.5% Quillaja 1%Castor, 34% 2.34 0.12 Water with 34% PG) Day 1 Sample C (0.5% Quillaja1%, 15% Water 2.55 0.13 with 53%) Day 1 Sample D (0.5% Quillaja 1%, 10%Water 2.47 0.16 with 58% PG) Day 1 Sample E (0.5% Quillaja 1%, 5% Water2.43 0.24 with 63% PG) Day 1

This Example shows that as more water was replaced with anothernon-aqueous liquid such as propylene glycol, the quillaja showedincreasingly enhanced stability relative to the control (Sample A) dueto propylene glycol's effect on the acidulants.

The emulsion-including beverage concentrates described herein areadvantageously stabilized by quillaja even at the low pH of 2.6 orbelow, thereby permitting the beverage concentrates to be shelf-stablefor about 12 months. The use of quillaja as a stabilizer in theemulsion-including beverage concentrates described herein advantageouslypermit the beverage concentrates not to include weighting agents,thereby reducing manufacturing costs. In addition, the presence of thenon-aqueous liquid in the beverage concentrates may slow the rate offlavor deterioration and provide for higher quality of flavor in thebeverage concentrate and/or the final beverage over a longer period oftime. In addition, the presence of the non-aqueous liquid in thebeverage concentrate may advantageously reduce the corrosiveness of thebeverage concentrate relative to the packaging due to a largerpercentage of the acid not being in its active state. Yet anotheradvantage of the beverage concentrates described herein is thatquillaja-stabilized emulsions may be more concentrated than conventionalemulsions, thereby saving on raw material costs and shipping costs.

The foregoing descriptions are not intended to represent the only formsof the concentrates in regard to the details of formulation. Thepercentages provided herein are by weight unless stated otherwise.Changes in form and in proportion of parts, as well as the substitutionof equivalents, are contemplated as circumstances may suggest or renderexpedient. Similarly, while beverage concentrates and methods have beendescribed herein in conjunction with specific embodiments, manyalternatives, modifications, and variations will be apparent to thoseskilled in the art in light of the foregoing description.

What is claimed is:
 1. A method of making a concentrate including anoil-in-water emulsion, the method comprising: providing a solutionincluding about 15% to about 70% non-aqueous solvent and about 2% toabout 60% acidulant; mixing quillaja, a lipid, and water to form a blendin a form of an oil-in-water emulsion including about 0.01% to about 20%quillaja, about 0.01% to about 60% lipid, about 0% to about 10% buffer,and about 1% to about 99% water; adding the blend in an amount of 0.1%to about 35% by total weight to the solution to form anemulsion-including concentrate having a pH of about 2.0 to about 2.6. 2.The method of claim 1, wherein the emulsion-including concentrateincludes about 0.01% to about 8% quillaja.
 3. The method of claim 1,wherein the non-aqueous solvent is selected from the group consisting ofpropylene glycol, glycerol, ethanol, triacetin, ethyl acetate, benzylalcohol, vegetable oil, 1,3-propanediol, and combinations thereof. 4.The method of claim 1, wherein the acidulant is an selected from thegroup consisting of citric acid, malic acid, succinic acid, acetic acid,adipic acid, tartaric acid, fumaric acid, phosphoric acid, lactic acid,salts thereof, and combinations thereof.
 5. The method of claim 1,wherein the lipid is selected from the group consisting of castor oil,terpene hydrocarbons, flavor oils (consisting of one or more of thefollowing derivatives: ketones, aldehydes, lactones, ethers, esters,sulfur compounds, furanones, terpenoids), oil soluble vitamins,nutraceuticals, fatty acids, poly-unsaturated fatty acids, triglyceridesand triglyceride derivatives, antioxidants, colorants, vegetable oils,and combinations thereof.
 6. The method of claim 1, further comprisingadding the blend to the solution to provide a ratio of the water to thenon-aqueous solvent in the emulsion concentrate from 6:1 to about 1:6and a ratio of the water to the acidulant in the emulsion concentrate isfrom about 60:1 to about 1:10.
 7. The method of claim 1, wherein thebuffer is selected from the group consisting of sodium, calcium orpotassium salts of citrate, malate, succinate, acetate, adipate,tartrate, fumarate, phosphate, lactate, or carbonate, and combinationsthereof.
 8. The method of claim 1, further comprising adding the blendto the solution to provide the emulsion-including concentrate includingwater in an amount of 30% or less.
 9. The method of claim 1, wherein theadding the blend to the solution does not include providing a weightingagent in the emulsion-including concentrate.
 10. The method of claim 1,wherein the adding the blend to the solution provides theemulsion-including concentrate that is shelf-stable at temperatures ofabout 20° C. to about 25° C. for about twelve months.